Yellow basic dye.



;' (UNITED STATES PATENT OFFICE. i

CARL OSCAR MllLLER, or BASLE, SWITZERLAND, Assieuonro run ,BADISOHE 'A ILIN AND soon FABRIK, or LUDWIGSHAFEN, era

MANY.

YELLOW BASICDYE.

SPECIFICATION forming part of Letters Patent No. 633,883, dated Septemb hpplication filed June 23, 1899. Serial in. 721,611- No Specimens) To all whmn it vita "concern:

Be it known that I, CARL Oscxn Mii LEn,

chemist, a subject of the King of Saxony, and

a resident of Basle, Switzerland, have in- 5 vented a new Yellow Basic Coloring-Matter,

said mother-liquid by acids.

of which the following is a clear, full, and exact specification.

If phthalie anhydride and a mono-alkylaied meta amido 5 phenol (mono-methylor monor ethyl-meta-amido-phenol) be heated together,

2o ered that it can by suitable treatment be converted into a new yellow basic coloring-matter soluble in water and possessing valuable dyeing properties.

The process by which I convert the said waste product into my new coloring-matters consists in first treating it with alcoholic hydrochloric acid, so as to remove all pitchy matters and convert it into a yellow crystalline intermediate product, which is but slightly soluble even in boiling water. If desired, the waste product can first be heated with an alkaline solution, say caustic soda, either at ordinary pressure or in an autoclave. After this treatment the action of the alcoholic hydrochloric acid need not be so prolonged as is otherwise the case. The crystalline intermediate product obtained as hereinbefore described is converted into my new coloring-matter by submitting it to cs- 40 ierification, for instance, by treatment with sulfuric acid and an alcohol.

The following example will serve to illustrate the manner inwhich my invention can be carried into effect and my new coloringmatter obtained: .Prepare adialkyhrhodamin melt in the well-known way from say ten parts mono-ethyl-meta-amido-phenol, ten (10) parts of phthalic anhydride, and five (5) parts chlorid of zinc. WVork up in theknown 50 way by washing with water and treating with ammonia and filter to separate therhodam'in base. (See United States Patent No. 456,081

To the mother-liquor add sufiicient acid to precipitate the by-product. Now mix together two hundred (200) parts of the said by-product, six hundred (600) parts of water, and two hundred (200) parts of caustic-soda lye, (containing thirty per cent. NaOH.) Heat this mixture for about seven hours to a temper-attire of from 150 to 160 centigrade in an autoclave. Then filter, and in order to precipitate the product add so much hydrochlo ric acid that a distinct excess thereof is present. Treat the precipitated product by boiling with one hundred and sixty (160) parts of alcohol, one hundred and fifty (L50) parts of water, and fifty (50) parts of hydrochloric acid, (containing twenty-nine per cent. H01.) Allow the mixture to cool to 60 and collect the crystals which separate by filtration. Wash the crystals with a mixture of alcohol, water, and hydrochloric acid in the aforesaid proportions repeatedly until no more pitchy admixtures are dissolved. Yellow crystals of the intermediate product are obtained in this way, which dissolve in alkalies, giving a greenly fluorescent solution. They are but slightly soluble in dilute acids. .To obtain my new coloring-matter, mix thirty parts of the crystals so obtained with eighty (80) parts of alcohol and severity (70) parts of sulfuric acid monohydrate. Heat this mixture for about six hours on the boiling-water bath until a clear solutionbe obtained. Allow the mixture to cool and run it into about seven hundred (700) parts of cold water, which is maintained alkaline by the addition of causticsoda lye throughout. Cool the liquid and so regulate therate of mixing that the temperature does not rise above, say, centigrade. The coloring-matter base separates out and is collected by filtration, washed with water, and treated in a centrifugal machine. Dissolve it in a boiling mixture of eighty (80) parts alcohol, eighty (80) parts of water, and

twenty (20) parts of hydrochloric acid. Ell-- ter in a closedvessel to free from insoluble impurities. Allow the mixture to cool to about cen'tigrade and add fifty parts fifty (50) parts waof hydrochloric acid and tor to completely precipitate the coloringmatter. When Lheseparation has taken place,

filter, press,and dry. If desired, Ishecoloring-malater can be purified by reorystallizing from W-falifil. i

My new coloring-matter dissolves in water,

giving orange-yellow solutions with greenish fluorescence, his also readily soluble in elbeautiful yellow shades.

oohol and in concentrated sulfuric acid. In clyesocot ton moi-denoted with tannin, giving It; is further oimro my name, this 8th day of; June, 1899, in presence of two subscribing witnesses.

05m be obtained from the lu -product; from the-action of phbhalic auhyd'ride with monoalkyl-meta-amido-phenol and whlch'is soluble in water giving a yellow fluorescent solution, and which, on treatment; with warm (lilute oaustiosoda solution, is converted into a yellow oryst alline product; almost; insoluble in dilute acids, soluble in alkalies giving a solution possessing a greenish fluorescence,

aillsubstanniallly as desorihed.

In witness; whereof I have her-eunfio signed CARL osoAR MI'JLLER.

' Witnesses:

GEORGE GIFFORD, "AMAND BITTER. 

